CN101805568A - Bio oil-starch adhesive and preparation method thereof - Google Patents
Bio oil-starch adhesive and preparation method thereof Download PDFInfo
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- CN101805568A CN101805568A CN 201010119029 CN201010119029A CN101805568A CN 101805568 A CN101805568 A CN 101805568A CN 201010119029 CN201010119029 CN 201010119029 CN 201010119029 A CN201010119029 A CN 201010119029A CN 101805568 A CN101805568 A CN 101805568A
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Abstract
The invention relates to a novel bio oil-starch adhesive for the artificial board and a preparation method thereof, which belong to the technical field of the artificial board in the wood processing. The adhesive uses starch and bio oil as the main raw material. The preparation method comprises the following steps: firstly carrying out acidolysis and oxidation treatment on the starch and simultaneously carrying out purification treatment on the bio oil; then carrying out proportioning on the processed bio oil and starch according to proper proportion and preparing linear high molecular polymer by addition and polycondensation reactions; adding polyvinyl alcohol into the high molecular polymer to prepare a main agent of the adhesive by esterification; and finally adding a borax cross-linking agent and diisocyanate into the main agent of the adhesive to prepare the bio oil-starch adhesive. The invention has the characteristics of novel design, standard process, no environment pollution and the like. The prepared adhesive has the advantages of environment protection, low cost, good water resisting property, high stability and the like and can be widely used in the fields of building materials, house decoration, home decoration and the like.
Description
Technical field
The invention belongs to man-made board technology field in the wood working, be specifically related to a kind of bio oil-starch adhesive and preparation method thereof.
Technical background
In recent years, to stick with glue the development trend of agent be environmental protection, with low cost, excellent property, save energy and solvent free direction to the wood-based plate industry.And on present wood-based plate market, three traditional aldehyde adhesive sticks (urea-formaldehyde resin adhesive, synvaren and melamine resin adehsive stick) are dominate still, because three aldehyde adhesive sticks easily discharge objectionable impuritiess such as formaldehyde, cause human health and society and nature's environment to be on the hazard, therefore the mankind press for and develop a kind of novel environment friendly tackiness agent at present, make it to realize eco-friendly purpose, can bring certain economic benefits to society again.In this case, starch-base timber adhesive arises at the historic moment.
Starch is natural high molecular polymer, has a large amount of hydroxyl isoreactivity groups, and this haves laid a good foundation for the preparation tackiness agent.Worked out multiple starch-base timber adhesive at present, (reference Wang Xin ripple such as Wang Xinbo, Wu Youshi. the preparation of urea-dialdehyde starch tackiness agent. meticulous and chemical special product, 2003,13.) at first starch is carried out the dialdehyde processing, then dialdehyde starch and the urea that makes is reacted under acidic conditions, add borax at last and carry out complexing, thereby make timber starch-based glue stick; Although its performance of tackiness agent of utilizing this method to prepare meets the GB requirement,, therefore still do not break away from the dependence of tackiness agent to fossil resource because its main raw material is a urea.(Shi Junyou such as Shi Junyou, Wang Shumin. the research of W-Gum modification API glue. Chinese tackiness agent, 2006,1.) earlier starch is carried out acidolysis, oxide treatment, under the effect of initiator ammonium persulfate, make composite modified starch with acrylamide graft, adding polyvinyl alcohol and starch generation esterification make starch adhesive host under the condition that oxalic acid exists then, add linking agent-polymeric isocyanate at last and prepare the wood-based plate starch adhesive; Adopt tackiness agent gummed intensity that this method prepares and water tolerance all than higher, but because its raw material is that W-Gum causes resource scarcity easily, being not suitable for big area promotes, the auxiliary reagent that adds in the preparation process of this tackiness agent is more in addition, complicated operation, thereby cause the preparation cost of tackiness agent higher, the market competitiveness is relatively poor.
Exhausted day by day along with the petrochemical industry resource, develop a kind of is that environmental protection, excellent property, the cheap novel adhesive of raw material become promote that wood industry develops necessary with the renewable resources.
Summary of the invention:
The objective of the invention is at above-mentioned deficiency, proposing to adopt starch and bio oil is main raw material, respectively starch is carried out acidolysis, oxide treatment, bio oil is made with extra care after the purification processes, both are reacted under acidic conditions, carry out grafting at the adding polyvinyl alcohol, add borax and isocyanate-crosslinked at last, make novel environment friendly starch glue for lumber stick.
The technical scheme that realizes the object of the invention is:
Bio oil-starch adhesive belongs to two component adhesive, and host, linking agent are made up of the raw material of following heavy constituent respectively:
Host:
Concentration is 100 parts of 35%～40% acidolysis, Sumstar 190s, 30～40 parts of refining biological oils, 50～150 parts of polyvinyl alcohol solutions, 30～40 parts of oxalic acid solution.
Complexing agent and solidifying agent:
20～30 parts of water-based vulcabond; 1.2～4.8 parts of boraxs.
Described concentration is that 35%～40% acid hydrolysis oxidative starch emulsion is made up of the raw material of following weight parts: 35～40 parts of tapioca (flour)s, and 60～65 parts of the mineral acids of concentration 0.3～0.5mol/L, concentration is 40～65 parts of the oxygenant sodium periodates of 0.6mol/L.In the used raw material of preparation acidolysis, Sumstar 190 emulsion, mineral acid can be hydrochloric acid or sulfuric acid; Polyvinyl alcohol solution is that concentration is 8% or 12% the aqueous solution; Oxalic acid is that concentration is 30% the aqueous solution.The NaOH of the PH conditioning agent 10% that uses in the preparation process or 5% hydrochloric acid.
Described linking agent water-based vulcabond is that concentration is 98% toluene diisocyanate.
The preparation method that above-mentioned each raw material is made bio oil-starch adhesive of the present invention is:
1. the acidolysis of starch, oxidation:
35-40 part tapioca (flour) is joined in the hydrochloric acid of 60～65 parts of concentration 0.3～0.5mol/L, be mixed with concentration and be 35%～40% starch emulsion, transfer PH to 1～2, this emulsion is joined in the there-necked flask of prolong and thermometer, be warmed up to 35 ℃～80 ℃ under keeping stirring, constant temperature acidolysis reaction 1～3 hour, transfer pH value to 5～6, add concentration then and be 40～65 parts of the sodium periodate solutions of 0.6mol/L, oxidizing reaction is 1～3 hour when temperature is 35 ℃-80 ℃, add an amount of sodium sulfite solution and stop oxidizing reaction, promptly make acid hydrolysis oxidative starch;
2. bio oil is refining purifies:
300 parts of bio oil are dissolved in 300 parts of ethyl acetate solutions, process filter paper removes by filter the coke part in the bio oil, mixture with bio oil and ethyl acetate leaves standstill for some time then, whole mixture is divided into A, B phase, A is rich in organic ethyl acetate part, and B is the part that is insoluble to ethyl acetate mutually; Tell the B phase with separating funnel, wash A phase solution repeatedly to remove some water miscible materials, then with the NaHCO of A phased soln at 300 part 5% with distilled water
3In the aqueous solution and mix, make organic acid substance and the reaction of sodium bicarbonate of A in mutually generate water miscible salt, A is divided into two portions again mutually like this, and a part is aldehydes matter and the neutral substance that is dissolved in ethyl acetate, and another part is water-soluble salt; Tell the salts substances of solution water again with separating funnel, the ethyl acetate solution that will contain aldehydes matter is at last removed solvent ethyl acetate and water-soluble substances successively with Rotary Evaporators, and surplus materials is the polyatomic phenol material;
3. prepare polyvinyl alcohol water solution, the oxalic acid aqueous solution:
Under agitation particulate polyethylene alcohol is added to the water, by warming-in-water to 80 ℃～95 ℃, insulation 30min～1h is dissolved in the water fully until polyvinyl alcohol, is cooled to 50 ℃ then, add an amount of ammonium persulphate oxidation 30min, make 8% or 12% polyvinyl alcohol solution; Get a certain amount of particulate state oxalic acid, add an amount of water by 30% concentration, be warming up to 50 ℃ under the stirring that does not stop, be incubated to oxalic acid and all dissolve, it is standby to reduce to room temperature;
4. prepare tackiness agent host:
Under agitation, transferring pH value is 2～5.5, add first (15～25 parts) refining biological oil in the starch solution of acid hydrolysis oxidative, insulation reaction 30～40min under 45 ℃～75 ℃ temperature, add second batch of remaining refining biological oil again in solution, insulation reaction 30～40min, transferring pH value is 9～10, is warming up to 45 ℃～80 ℃, evenly imports polyvinyl alcohol solution 50-150 part then in 20min, alternately add alkali lye and oxalic acid every 10min then, so repeatable operation till oxalic acid adds, adds sodium sulphite anhydrous 99.3 reduction excess oxidant, transferring pH value again is 7, is cooled to 50 ℃;
5. add complexing agent:
Under constantly stirring, add 1.2～4.8 parts of boraxs, till viscosity reaches requirement.
6. add solidifying agent and filler:
In the starch adhesive host of above-mentioned preparation, add 20～30 parts of toluene diisocyanates and constantly stirring, till both mix fully; Add filler flour and light calcium carbonate powder at last, make the solids content of tackiness agent reach 48%～52%.
The present invention has positive effect:
1. outstanding feature of the present invention is that natural wild tapioca (flour) and the agricultural residuum fast pyrogenation bio oil of employing is that main raw material prepares wood adhesive, need not to use formaldehyde, the formaldehyde that has not only fundamentally solved three aldehyde adhesive sticks discharges problem, and has realized effective utilization of wild cassava resource and agricultural residuum resource.
2. used polyvinyl alcohol water solution is made in water by the polyvinyl alcohol heating for dissolving among the present invention, and the aqueous solution of polyvinyl alcohol is nontoxic material; Content in the more similar amylan of used curing agent toluene-diisocyanate content is few, and therefore the tackiness agent toxicity of preparation is little, free from environmental pollution, also can not damage human body, belongs to the tackiness agent of environmental type.
3. the required reaction conditions gentleness of preparation process of the present invention, easy and simple to handle, and equipment is easy to get, implement easily.
4. tackiness agent of the present invention can be used for the bonding of woodwork by coating method, wherein bio oil and starch and polyvinyl alcohol and starch, toluene diisocyanate form the reticulated structure that mutually combines, even if so these goods are put into water, can not come off in its bonded part yet, so product of the present invention has the better waterproof energy.
Concrete embodiment:
Embodiment 1
1. the acidolysis of starch, oxidation:
35 parts of tapioca (flour) parts are joined in the hydrochloric acid of 65 parts of concentration 0.5mol/L, be mixed with concentration and be 35% starch emulsion, transfer PH to 2, this emulsion is joined in the there-necked flask of prolong and thermometer, be warmed up to 50 ℃ under keeping stirring, constant temperature acidolysis reaction 3 hours, transfer pH value to 4～6, add concentration then and be 65 parts of the sodium periodate solutions of 0.6mol/L, oxidizing reaction is 3 hours when temperature is 35 ℃, add an amount of sodium sulfite solution and stop oxidizing reaction, promptly make acid hydrolysis oxidative starch;
2. the refining purification of bio oil:
100 parts of bio oil crude oil are dissolved in 100 parts of ethyl acetate solutions, process filter paper removes by filter the coke part in the bio oil, mixture with bio oil and ethyl acetate leaves standstill for some time then, whole mixture is divided into A, B phase, A is rich in organic ethyl acetate part, and B is the part that is insoluble to ethyl acetate mutually; Tell the B phase with separating funnel, wash A phase solution repeatedly to remove some water miscible materials, then with the NaHCO of A phased soln at 50 part 5% with distilled water
3In the aqueous solution and mix, make organic acid substance and the reaction of sodium bicarbonate of A in mutually generate water miscible salt, A is divided into two portions again mutually like this, and a part is aldehydes matter and the neutral substance that is dissolved in ethyl acetate, and another part is water-soluble salt; Tell the salts substances of solution water again with separating funnel, the ethyl acetate solution that will contain aldehydes matter is at last removed solvent ethyl acetate and water-soluble substances successively with Rotary Evaporators, and surplus materials is the polyatomic phenol material;
3. prepare tackiness agent host:
Under continuous stirring condition, transferring pH value is 4, add first refining biological oil (account for essential oil total amount 60%) in the starch solution of acid hydrolysis oxidative, insulation reaction 30min under 55 ℃ temperature, add second batch of remaining refining biological oil again in solution, insulation reaction 30min, in 20min, evenly import concentration then and be 50 parts of 12% polyvinyl alcohol solutions, in 120min, alternately add alkali lye and oxalic acid then every 10min, so repeatable operation till oxalic acid adds, adds S-WAT reduction excess oxidant, transferring PH is 7, is cooled to 50 ℃;
4. add complexing agent and solidifying agent:
Add 4 parts of boraxs under constantly stirring, till viscosity reaches requirement; In the starch adhesive host of above-mentioned preparation, add 30 parts of toluene diisocyanates and constantly stirring, till both mix fully; Add suitable filler light calcium carbonate powder at last, stir, be cooled to room temperature, obtain the bio oil-starch adhesive that a kind of wood-based plate is used.
Embodiment 2
The step 1. consumption of middle tapioca (flour) is 40 parts, and the consumption of hydrochloric acid is 60 parts, and the acidolysis reaction temperature is 35 ℃; The temperature of reaction of 3. middle bio oil of step and starch is 65 ℃, and the reaction times is 40min, is warming up to 80 ℃, and the amount of the polyvinyl alcohol of adding is 100 parts of reaction 50min; Other raw materials and reaction conditions are as embodiment 1.
Embodiment 3
The temperature of 1. middle acidolysis of step and oxidizing reaction is 80 ℃, and the time of acidolysis and oxidizing reaction is 1 hour; Step 3. bio oil and starch reaction temperature is 75 ℃, and the amount that adds polyvinyl alcohol solution is 150 parts; The 4. middle amount that adds borax of step is 2 parts, and the amount of isocyanic ester is 20 parts; Other raw materials and reaction conditions are as embodiment 1.
Embodiment 4
The step 3. amount of middle refining biological oil is 40 parts, and bio oil is once to add; The 4. middle filler of step is a flour; Other raw materials and reaction conditions are as embodiment 1.
Claims (11)
1. the preparation method of a bio oil-starch adhesive, may further comprise the steps: the 1. acidolysis of starch, oxidation: starch emulsion is joined in the there-necked flask of prolong and thermometer, be warmed up to 35 ℃～80 ℃ under keeping stirring, add an amount of hydrochloric acid, transfer PH=1～2, constant temperature acidolysis reaction 1～3 hour, add sodium periodate solution then, oxidizing reaction is 1～3 hour when temperature is 35 ℃～80 ℃, add an amount of sodium sulfite solution and stop oxidizing reaction, promptly make acid hydrolysis oxidative starch; 2. bio oil is refining purifies: the mass ratio of bio oil according to 1: 1 is dissolved in the ethyl acetate solution, process filter paper removes by filter the coke part in the bio oil, mixture with bio oil and ethyl acetate leaves standstill for some time then, whole mixture is divided into A, B phase, A is rich in organic ethyl acetate part, and B is the part that is insoluble to ethyl acetate mutually; Wash A phase solution repeatedly to remove some water miscible materials with distilled water, then with the A phased soln at 5% NaHCO
3In the aqueous solution and mix, make organic acid substance and the reaction of sodium bicarbonate of A in mutually generate water miscible salt, A is divided into two portions again mutually like this, and a part is aldehydes matter and the neutral substance that is dissolved in ethyl acetate, and another part is water-soluble salt; Remove solvent ethyl acetate and water-soluble substances successively with Rotary Evaporators at last, surplus materials is the polyatomic phenol material; 3. prepare the polyvinyl alcohol water solution and the oxalic acid aqueous solution: under agitation particulate polyethylene alcohol is added to the water, by warming-in-water to 95 ℃, be cooled to 50 ℃ behind the insulation 1h, add Potassium Persulphate oxidation 30min, make 8%～12% polyvinyl alcohol solution; Get a certain amount of oxalic acid, add an amount of water by 30% concentration, be warming up to 50 ℃ under the stirring that does not stop, be incubated to oxalic acid and all dissolve, it is standby to reduce to room temperature; 4. prepare tackiness agent host: under agitation, transfer pH value to 2～5.5, add the 2. middle refining biological oil for preparing of first step then in the starch solution of acid hydrolysis oxidative, insulation reaction 30～40min under 45 ℃～75 ℃ temperature, add second batch of refining biological oil again, insulation reaction 30～40min transfers PH to 9～10, is warming up to 45 ℃～80 ℃, the polyvinyl alcohol solution of preparation in 20min, evenly importing 3. again, alternately add alkali lye and oxalic acid then, repeatable operation like this is till oxalic acid adds, add sodium sulphite anhydrous 99.3, the reduction excess oxidant, transferring pH value with acetate again is 7, is cooled to 50 ℃; 5. in the host of above-mentioned preparation, add complexing agent-borax, be warming up to 80 ℃～90 ℃ and continuation stirring 0.5h～1h, until borax and the abundant gelatinization of host, crosslinked; 6. be cooled to 50 ℃～80 ℃, under whipped state, add solidifying agent-vulcabond, mix to both; Last filled impregnation stick solids content is 48%～52%, is cooled to normal temperature, obtains a kind of bio oil-starch adhesive of environmental type.
2. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that the starch source during step 1. is wild tapioca (flour).
3. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that the massfraction of starch emulsion was 35%～40% during step 1..
4. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that the temperature of starch emulsion acidolysis was 35 ℃～80 ℃ during step 1.; The temperature of oxidation is 35 ℃～80 ℃.
5. the preparation method of bio oil-starch adhesive according to claim 1, it is characterized in that step 1. the concentration of meso-periodic acid sodium be 0.6mol/L, and the mol ratio of itself and starch is 1～1.1: 1.
6. the preparation method of bio oil-starch adhesive according to claim 1, its feature step 2. in employed bio oil be the agricultural residuum fast pyrogenation bio oil of Beijing Forestry University's Materials Academy independent development.
7. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that during step 4. it being that the ph value of reaction of bio oil and starch is 2～5.5.
8. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that the temperature of reaction of 4. middle refining biological oil of step and treated starch is 45 ℃～75 ℃.
9. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that the quality of the complexing agent-borax of adding during step 5. accounts for 0.5%～2% of tackiness agent host quality.
10. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that the quality of the solidifying agent-isocyanic ester of adding during step 6. accounts for 8%～12% of tackiness agent host quality.
11. the preparation method of bio oil-starch adhesive according to claim 1 is characterized in that the filler that adds during step 6. is flour and light calcium carbonate powder.
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Cited By (11)
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| CN102010678A (en) * | 2010-09-30 | 2011-04-13 | 北京林业大学 | Preparation method for biological oil-phenol-starch adhesive |
| CN102634298A (en) * | 2012-05-03 | 2012-08-15 | 北京林业大学 | Biological oil-starch-glyoxal resin adhesive for artificial board and preparation method of biological oil-starch-glyoxal resin adhesive |
| CN102642222A (en) * | 2012-05-03 | 2012-08-22 | 北京林业大学 | Method for preparing aldehyde-free veneer boards by biological oil starch adhesives |
| CN103122228A (en) * | 2013-03-01 | 2013-05-29 | 北京林业大学 | Bio-oil starch adhesive for wood and preparation method |
| CN104910839A (en) * | 2015-06-16 | 2015-09-16 | 北京林业大学 | Regulation and control method for preparation process for bio-oil starch adhesive for wood |
| US9167662B2 (en) | 2012-02-29 | 2015-10-20 | Cirrus Logic, Inc. | Mixed load current compensation for LED lighting |
| US9184661B2 (en) | 2012-08-27 | 2015-11-10 | Cirrus Logic, Inc. | Power conversion with controlled capacitance charging including attach state control |
| US9307601B2 (en) | 2010-08-17 | 2016-04-05 | Koninklijke Philips N.V. | Input voltage sensing for a switching power converter and a triac-based dimmer |
| CN105646723A (en) * | 2016-03-30 | 2016-06-08 | 中南林业科技大学 | Dialdehyde starch and preparation method thereof |
| CN108641633A (en) * | 2018-05-18 | 2018-10-12 | 胡果青 | A kind of preparation method of water-resistant type carton adhesive |
| CN109593508A (en) * | 2018-12-19 | 2019-04-09 | 山东农业大学 | A kind of wood-based plate biology base is without aldehyde adhesive and preparation method thereof |
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| US9307601B2 (en) | 2010-08-17 | 2016-04-05 | Koninklijke Philips N.V. | Input voltage sensing for a switching power converter and a triac-based dimmer |
| CN102010678A (en) * | 2010-09-30 | 2011-04-13 | 北京林业大学 | Preparation method for biological oil-phenol-starch adhesive |
| US9167662B2 (en) | 2012-02-29 | 2015-10-20 | Cirrus Logic, Inc. | Mixed load current compensation for LED lighting |
| CN102634298A (en) * | 2012-05-03 | 2012-08-15 | 北京林业大学 | Biological oil-starch-glyoxal resin adhesive for artificial board and preparation method of biological oil-starch-glyoxal resin adhesive |
| CN102642222A (en) * | 2012-05-03 | 2012-08-22 | 北京林业大学 | Method for preparing aldehyde-free veneer boards by biological oil starch adhesives |
| CN102642222B (en) * | 2012-05-03 | 2015-06-17 | 北京林业大学 | Method for preparing aldehyde-free veneer boards by biological oil starch adhesives |
| US9184661B2 (en) | 2012-08-27 | 2015-11-10 | Cirrus Logic, Inc. | Power conversion with controlled capacitance charging including attach state control |
| CN103122228A (en) * | 2013-03-01 | 2013-05-29 | 北京林业大学 | Bio-oil starch adhesive for wood and preparation method |
| CN103122228B (en) * | 2013-03-01 | 2014-12-10 | 北京林业大学 | Bio-oil starch adhesive for wood and preparation method |
| CN104910839A (en) * | 2015-06-16 | 2015-09-16 | 北京林业大学 | Regulation and control method for preparation process for bio-oil starch adhesive for wood |
| CN105646723A (en) * | 2016-03-30 | 2016-06-08 | 中南林业科技大学 | Dialdehyde starch and preparation method thereof |
| CN105646723B (en) * | 2016-03-30 | 2018-09-07 | 中南林业科技大学 | A kind of dialdehyde starch and preparation method thereof |
| CN108641633A (en) * | 2018-05-18 | 2018-10-12 | 胡果青 | A kind of preparation method of water-resistant type carton adhesive |
| CN109593508A (en) * | 2018-12-19 | 2019-04-09 | 山东农业大学 | A kind of wood-based plate biology base is without aldehyde adhesive and preparation method thereof |
| CN109593508B (en) * | 2018-12-19 | 2020-05-12 | 山东农业大学 | Bio-based formaldehyde-free adhesive for artificial board and preparation method thereof |
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Open date: 20100818 |